TiB2-containing　nano-microstructured　feedstock　was　prepared　by　spray-drying　and　vacuum　heat-treatment.　X-ray　diffraction,　scanning　electron　microcopy,　laser　diffraction　were　applied　to　characterize　the　agglomerated　particles.　The　experimental　results　show　that　the　shape,　the　distribution　of　particles　size,　and　the　flowability　of　the　agglomerated　particles　are　suitable　for　thermal　spraying.　The　composition　of　the　original　powder　has　not　changed　after　vacuum　heat　treatment,　the　densified　TiB2　composite　coating　can　be　fabricated　by　axial　plasma　spraying　(Mettech　Axial-III)　using　nano-microstructured　feedstock　prepared　by　spray-drying　followed　by　vacuum　heat-treatment.